CN102674481A - Process for preparing ferrous sulfate solution by removing impurities from steel pickling waste liquid - Google Patents
Process for preparing ferrous sulfate solution by removing impurities from steel pickling waste liquid Download PDFInfo
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- CN102674481A CN102674481A CN201210191474XA CN201210191474A CN102674481A CN 102674481 A CN102674481 A CN 102674481A CN 201210191474X A CN201210191474X A CN 201210191474XA CN 201210191474 A CN201210191474 A CN 201210191474A CN 102674481 A CN102674481 A CN 102674481A
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Abstract
The invention discloses a process for preparing a ferrous sulfate solution by removing impurities from steel pickling waste liquid. The process comprises the following steps of measuring the concentration of ferrous sulfate, sulfuric acid, an impurity element in a waste sulfuric acid solution; adding a certain amount of water into the obtained waste sulfuric acid solution, so that concentration of the reacted ferrous sulfate solution is 25 to 35 weight percent; adding a sufficient number of iron shavings according to the measured concentration of the residual sulfuric acid, and fully reacting the sulfuric acid with the iron shavings to produce the ferrous sulfate so as to obtain the ferrous sulfate solution without residual acid; heating to 50 to 60 DEG C, and keeping the temperature for 2 to 3h until the pH is more than or equal to 3; continuously heating to 90 to 100 DEG C, keeping the temperature for 2 to 3h until the pH is 4 to 5, stopping heating, standing, and cooling until a precipitate is not separated out; filtering, testing and storing for use. By the process, the ferrous sulfate solution which can be used for preparing iron black is prepared; the process is favorable for environment protection; the waste treatment cost is saved; new economic benefits are created; and the process is suitable for large-scale popularization and application.
Description
Technical field
The present invention relates to the technology that the removal of impurities of a kind of acid washing rolled steel waste liquid prepares copperas solution.
Background technology
Steel Mill can produce a large amount of sulfur waste acid in pickling blank process; Wherein contain a large amount of ferrous sulfate; Ferrous sulfate can be used for iron black preparation technology, but owing to also contain other a large amount of impurity simultaneously in the spent acid, such as Cl, Cr, S, C, Mo, S, P, Cu, Mn plasma; If detrimental impurity is not wherein removed, be to realize fully being used for iron black preparation technology's.Therefore, a large amount of spent acid can not get handling, and not only causes a large amount of wastings of resources, and causes environmental pollution.
Therefore, study the detrimental impurity of how removing in the sulfur waste acid and just become the significant work of ten minutes.
Summary of the invention
The object of the present invention is to provide the removal of impurities of a kind of acid washing rolled steel waste liquid to prepare the technology of copperas solution; Be used for when handling the acid washing rolled steel waste liquid, making the copperas solution that can be applicable to that preparation is iron black; The purpose that realization kills two birds with one stone; In the protection environment, economize on resources, produce additional economic benefit.
For this reason, technical scheme of the present invention is following:
The removal of impurities of a kind of acid washing rolled steel waste liquid prepares the technology of copperas solution, may further comprise the steps:
(1) measure the concentration of concentration, sulfuric acid concentration and the impurity element of ferrous sulfate in the sulfur waste acid, in the gained waste sulfuric acid solution, add a certain amount of water, the concentration that makes the copperas solution that end reaction finishes is to 25wt%-35wt%;
(2) add capacity iron plane flower according to the residual sulphur acid concentration that records, make all reacted ferrous sulfate with it of sulfuric acid, do not contain the copperas solution of residual acid;
(3) sulfur waste acid-respons process: be warming up to 50-60 ℃, constant temperature 2-3h to pH >=3;
(4) throw out cementation reaction process: continue to be warming up to 90-100 ℃, constant temperature 2-3h to pH is that 4-5 stops to heat, and the foreign ion replacement(metathesis)reaction in iron plane flower and the solution constantly has deposition to separate out in this process, leaves standstill to be cooled to no longer include to precipitate to separate out;
(5) filter, check stores for use.
Said impurity element comprises Cr, Mo, C, Si, P, Cu, Mn, V, Zn, Ni, Nb and Sn.
Finally, ferrous sulfate concentration is at 25wt%-35wt%, pH >=4, and color is a grass green, impurity content is judged to be salable product less than 0.05wt% person.
Committed step in the such scheme is useless vitriolic configuration, and before the reaction, the aimed concn value through thin up control reaction back copperas solution is between 25wt%-35wt%, and as not adding concentration control before the reaction beginning, the process inclusion-free is separated out.
Impurity element is separated out in temperature-rise period, its former because: iron plane flower generates ferrous sulfate with the sulfuric acid oxidation reaction.After sulfuric acid reaction finishes, be 90-100 ℃, PH >=4 in temperature, when concentration is 25wt%-35wt%, the foreign metal ion generation replacement(metathesis)reaction in iron plane flower and the solution makes foreign ion be replaced into throw out and separates out.
Pass through such scheme; The present invention has successfully realized removing the detrimental impurity element in the sulfur waste acid, has prepared with sulfur waste acid to can be used in the iron black copperas solution of preparation, turns waste into wealth; Not only help environment protection; And practiced thrift the waste disposal cost, and created new economic benefit, suit to apply on a large scale.
Embodiment
Embodiment:
(1) hand over the laboratory to measure the concentration of ferrous sulfate in the sulfur waste acid and the concentration of sulfuric acid concentration and impurity element the sulfur waste acid that receives; Recording ferrous sulfate concentration is 10wt%; Sulfuric acid concentration is 16wt%; Get the above-mentioned spent acid of 1000kg (as not adding water, the ferrous sulfate concentration for preparing will be 58wt%);
(2) add 1000kg water, dilution (after the dilution, the ferrous sulfate concentration that makes will be 29wt%);
(3) add 200kg iron plane flower (excessive), make all reacted ferrous sulfate with it of sulfuric acid;
(4) be warming up to 50 ℃, constant temperature 3h, recording pH is 3.5;
(5) continue to be warming up to 90 ℃, constantly have deposition to separate out in this process, constant temperature 2h, recording pH is 5, stops to heat, and leaves standstill to be cooled to no longer include to precipitate to separate out;
(4) filter, check, recording ferrous sulfate concentration is 28.3wt%, and pH is 5, and color is a grass green, is judged to be salable product, stores for use.
Table 1 is the detected result of each element in the detected result of each element in the sulfur waste acid of being adopted in the present embodiment and the prepared copperas solution.
Table 1 (wt% of unit)
Can find out that by above result it is fairly obvious that the present invention removes the effect of impurity.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment.So everyly do not break away from the equivalence of accomplishing under the disclosed spirit of the present invention or revise, all fall into the scope of the present invention's protection.
Claims (3)
1. acid washing rolled steel waste liquid removal of impurities prepares the technology of copperas solution, it is characterized in that, may further comprise the steps:
(1) measure the concentration of concentration, sulfuric acid concentration and the impurity element of ferrous sulfate in the sulfur waste acid, in the gained waste sulfuric acid solution, add a certain amount of water, the concentration that makes the copperas solution that end reaction finishes is to 25wt%-35wt%;
(2) add capacity iron plane flower according to the residual sulphur acid concentration that records, make all reacted ferrous sulfate with it of sulfuric acid, do not contain the copperas solution of residual acid;
(3) sulfur waste acid-respons process: be warming up to 50-60 ℃, constant temperature 2-3h to pH >=3;
(4) throw out cementation reaction process: continue to be warming up to 90-100 ℃, constant temperature 2-3h to pH is that 4-5 stops to heat, and the foreign ion replacement(metathesis)reaction in iron plane flower and the solution constantly has deposition to separate out in this process, leaves standstill to be cooled to no longer include to precipitate to separate out;
(5) filter, check stores for use.
2. the removal of impurities of the described acid washing rolled steel waste liquid of claim 1 prepares the technology of copperas solution, it is characterized in that said impurity element comprises Cr, Mo, C, Si, P, Cu, Mn, V, Zn, Ni, Nb and Sn.
3. the removal of impurities of the described acid washing rolled steel waste liquid of claim 1 prepares the technology of copperas solution, it is characterized in that ferrous sulfate concentration is at 25wt%-35wt%; It is 90-100 ℃ that foreign ion is separated out temperature; PH >=4, color is a grass green, impurity content is judged to be salable product less than 0.05wt% person.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210191474XA CN102674481A (en) | 2012-06-11 | 2012-06-11 | Process for preparing ferrous sulfate solution by removing impurities from steel pickling waste liquid |
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| CN201210191474XA CN102674481A (en) | 2012-06-11 | 2012-06-11 | Process for preparing ferrous sulfate solution by removing impurities from steel pickling waste liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107954480A (en) * | 2017-12-18 | 2018-04-24 | 东北大学 | A kind of sludge extraction iron of iron content containing zinc and the method for preparing iron oxide |
| CN109133450A (en) * | 2018-08-10 | 2019-01-04 | 天津城建大学 | A method of iron oxide black pigment is prepared using steel pickling waste liquor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857992A (en) * | 2006-05-29 | 2006-11-08 | 冶金部建筑研究总院上海分院 | Regenerating acid method by sulfuric acid substitution |
-
2012
- 2012-06-11 CN CN201210191474XA patent/CN102674481A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857992A (en) * | 2006-05-29 | 2006-11-08 | 冶金部建筑研究总院上海分院 | Regenerating acid method by sulfuric acid substitution |
Non-Patent Citations (2)
| Title |
|---|
| 李忠刚等: "酸洗废液回收回用工艺技术研究", 《有色矿冶》, vol. 20, no. 4, 31 August 2004 (2004-08-31) * |
| 樊盛春等: "钢铁酸洗废液的处理与综合利用", 《江西冶金》, vol. 20, no. 3, 30 June 2000 (2000-06-30), pages 12 - 14 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107954480A (en) * | 2017-12-18 | 2018-04-24 | 东北大学 | A kind of sludge extraction iron of iron content containing zinc and the method for preparing iron oxide |
| CN109133450A (en) * | 2018-08-10 | 2019-01-04 | 天津城建大学 | A method of iron oxide black pigment is prepared using steel pickling waste liquor |
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Effective date of abandoning: 20120919 |
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